Detection and correction of the misplacement error in THz Spectroscopy by application of singly subtractive Kramers-Kronig relations

In THz reflection spectroscopy the complex permittivity of an opaque medium is determined on the basis of the amplitude and of the phase of the reflected wave. There is usually a problem of phase error due to misplacement of the reference sample. Such experimental error brings inconsistency between phase and amplitude invoked by the causality principle. We propose a rigorous method to solve this relevant experimental problem by using an optimization method based upon singly subtractive Kramers-Kronig relations. The applicability of the method is demonstrated for measured data on an n-type undoped (100) InAs wafer in the spectral range from 0.5 up to 2.5 THz.Comment: 16 pages, 5 figure

On the role of API in determining porosity, pore structure and bulk modulus of the skeletal material in pharmaceutical tablets formed with MCC as sole excipient

The physical properties and mechanical integrity of pharmaceutical tablets are of major importance when loading with active pharmaceutical ingredient(s) (API) in order to ensure ease of processing, control of dosage and stability during transportation and handling prior to patient consumption. The interaction between API and excipient, acting as functional extender and binder, however, is little understood in this context. The API indomethacin is combined in this study with microcrystalline cellulose (MCC) at increasing loading levels. Tablets from the defined API/MCC ratios are made under conditions of controlled porosity and tablet thickness, resulting from different compression conditions, and thus compaction levels. Mercury intrusion porosimetry is used to establish the accessible pore volume, pore size distribution and, adopting the observed region of elastic intrusion-extrusion at high pressure, an elastic bulk modulus of the skeletal material is recorded. Porosity values are compared to previously published values derived from terahertz (THz) refractive index data obtained from exactly the same tablet sample sets. It is shown that the elastic bulk modulus is dependent on API wt% loading under constant tablet preparation conditions delivering equal dimensions and porosity. The findings are considered of novel value in respect to establishing consistency of tablet production and optimisation of physical properties

PHOTON MIGRATION IN PULP AND PAPER

Abstract The thesis clearly demonstrates that photon migration measurements allow characterization of pulp and paper properties, especially the fines and filler content of pulp, and the basis weight, thickness and porosity of paper. Pulp and paper are materials with a worldwide significance. Their properties strongly depend on the manufacturing process used. For efficient process control, the employed monitoring and measuring has to be fast. Therefore it is worthwhile to try to develop new approaches and techniques for such measurements. Recent advancements in optics offer new possibilities for such development. If two samples have different optical properties their photon migration distributions are different. The measurement of a photon migration distribution allows some features between two optically slightly dissimilar samples to be distinguished. Some simple measurements, which only yielded the photons' average time of flight, were made with an oscilloscope and a time-of-flight lidar. More precise measurements yielding photon pathway distribution or some selected characteristics like light pulse rise time, broadening, or fall time were measured with a streak camera. Two methods to assess photon path length distribution were introduced: particle determination with simulation, and streak camera with deconvolution. The basic properties for pulp are consistency and fines content and for paper the basic properties are thickness, basis weight and porosity. The influence on photon migration caused by changes in these basic properties was determined. As pulp and paper are rarely very basic, an additional property was demonstrated for both materials. For pulp it was the content of filler talc, and for paper it was the use of beaten pulp as a raw material. These additional properties were also distinguishable

Analysis of anisotropic pore structures using terahertz spectroscopy and imaging

This study demonstrates the analysis of anisotropic pore structures of highly porous pharmaceutical powder compacts by combining terahertz time-domain spectroscopy and in-situ measurements of the liquid penetration using terahertz pulsed imaging

A structure parameter for porous pharmaceutical tablets obtained with the aid of Wiener bounds for effective permittivity and terahertz time-delay measurement.

A structure parameter that can be used to predict the pattern of arrangement of porous inclusions in pharmaceutical tablets is introduced. By utilizing the effective refractive index of a pharmaceutical tablet obtained from terahertz time-domain measurements, we have shown that there exists a promising correlation between the calculated structural parameter and the porosity of training sets of pharmaceutical tablets, having well-defined characterization. Knowing of the structural arrangement, i.e. combined constituent skeletal-pore elements in series, parallel or mixed within porous media, could serve as a basis for understanding the ingress and permeation of liquids in such media. In the realm of pharmaceutical applications, such knowledge of the structural arrangement of air voids within a medicinal tablet could enable correlation with mechanical strength and dissolution behaviour in aqueous systems.This is the author accepted manuscript. The final version is available from Elsevier via http://dx.doi.org/10.1016/j.ijpharm.2016.04.02

Simultaneous investigation of the liquid transport and swelling performance during tablet disintegration.

Fast disintegrating tablets have commonly been used for fast oral drug delivery to patients with swallowing difficulties. The different characteristics of the pore structure of such formulations influence the liquid transport through the tablet and hence affect the disintegration time and the release of the drug in the body. In this work, terahertz time-domain spectroscopy and terahertz pulsed imaging were used as promising analytical techniques to quantitatively analyse the impact of the structural properties on the liquid uptake and swelling rates upon contact with the dissolution medium. Both the impact of porosity and formulation were investigated for theophylline and paracetamol based tablets. The drug substances were either formulated with functionalised calcium carbonate (FCC) with porosities of 45% and 60% or with microcrystalline cellulose (MCC) with porosities of 10% and 25%. The terahertz results reveal that the rate of liquid uptake is clearly influenced by the porosity of the tablets with a faster liquid transport observed for tablets with higher porosity, indicating that the samples exhibit structural similarity in respect to pore connectivity and pore size distribution characteristics in respect to permeability. The swelling of the FCC based tablets is fully controlled by the amount of disintegrant, whereas the liquid uptake is driven by the FCC material and the interparticle pores created during compaction. The MCC based formulations are more complex as the MCC significantly contributes to the overall tablet swelling. An increase in swelling with increasing porosity is observed in these tablets, which indicates that such formulations are performance-limited by their ability to take up liquid. Investigating the effect of the microstructure characteristics on the liquid transport and swelling kinetics is of great importance for reaching the next level of understanding of the drug delivery, and, depending on the surface nature of the pore carrier function, in turn controlling the performance of the drug mainly in respect to dissolution in the body

Sorting microplastics from other materials in water samples by ultra-high-definition imaging

In this study a commercial particle analyzer was used to image and help sorting microplastic particles (MPs) dispersed in filtrated and de-aerated tap water. The device provides a relatively easy and fast procedure for obtaining ultra-high-definition imaging, allowing the determination of shape, size, and number of 2D-projections of solid particles. The image analysis revealed clear differences among the studied different MPs originating from the grinding of five common grades of plastic sheets as they affect the image rendering differently, principally due to the light scattering either at the surface or in the volume of the microplastics. The high-quality imaging of the device also allows the discrimination of the microplastics from air bubbles with well-defined spherical shapes as well as to obtain an estimate of the size of MPs in a snapshot. We associate the differences among the shapes of the identified MPs in this study depending on the plastic type with known physical properties, such as brittleness, crystallinity, or softness. Furthermore, as a novel method we exploit a parameter based on the light intensity map from moving particles in cuvette flow to sort MPs from other particles, such as, wood fiber, human hair, and air bubbles. Using the light intensity map, which is related to the plastic-water refractive index ratio, the presence of microplastics in water can be revealed among other particles, but not their specific plastic type

Investigating elastic relaxation effects on the optical properties of functionalised calcium carbonate compacts using optics-based Heckel analysis

Heckel analysis is a widely used method for the characterisation of the compression behaviour of pharmaceutical samples during the preparation of solid dosage formulations. The present study introduces an optical version of the Heckel equation that is based on a combination of the conventional Heckel equation together with the linear relationship defined between the effective terahertz (THz) refractive index and the porosity of pharmaceutical tablets. The proposed optical Heckel equation allows us to, firstly, calculate the zero-porosity refractive index, and, secondly, predict the in-die development of the effective refractive index as a function of the compressive pressure during tablet compression. This was demonstrated for five batches of highly porous functionalised calcium carbonate (FCC) excipient compacts. The close match observed between the estimated in-die effective refractive index and the measured/out-of-die effective THz refractive index supports the validity of the proposed form of the equation. By comparing the measured and estimated in-die tablet properties, a clear change in the porosity and hence, the effective refractive index, due to post-compression elastic relaxation of the FCC compacts, has been observed. We have, therefore, proposed a THz-based compaction setup that will permit in-line monitoring of processes during tablet compression. We envisage that this new approach in tracking powder properties introduced in this preliminary study will lead to the onset of further extensive and detailed future studies